2,4-Dichloro-6-methoxy-3,5-triazine → 4-Chloro-6-methoxy-N-{2-[4-(trifluoromethoxy)phenyl]ethyl}-1,3,5-triazin-2-amine

HRID 517483

反応式

HRID 517483 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4]([O:9][CH3:10])[N:3]=1.CCN(C(C)C)C(C)C.[F:20][C:21]([F:33])([F:32])[O:22][C:23]1[CH:28]=[CH:27][C:26]([CH2:29][CH2:30][NH2:31])=[CH:25][CH:24]=1>C(#N)C>[Cl:8][C:6]1[N:5]=[C:4]([O:9][CH3:10])[N:3]=[C:2]([NH:31][CH2:30][CH2:29][C:26]2[CH:25]=[CH:24][C:23]([O:22][C:21]([F:20])([F:32])[F:33])=[CH:28][CH:27]=2)[N:7]=1

参加物

5

反応物 3

HCID 192672,4-Dichloro-6-methoxy-3,5-triazineHCID 81531DiisopropylethylamineHCID 106320402-[4-(Trifluoromethoxy)phenyl]ethan-1-amine

生成物 1

HCID 896196194-Chloro-6-methoxy-N-{2-[4-(trifluoromethoxy)phenyl]ethyl}-1,3,5-triazin-2-amine収率 90.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 5 g of 2,4-dichloro-6-methoxy-1,3,5-triazine in 50 ml of acetonitrile is cooled on an ice bath, 3.55 ml of DIPEA and then 5.13 g of 2-[4-(trifluoromethoxy)phenyl]ethanamine are added and the mixture is stirred for 30 minutes. The reaction mixture is partially concentrated under vacuum, an EtOAc/water mixture is added, the phases are separated by settling, the organic phase is washed with saturated NaCl solution and dried over MgSO4, and the solvent is evaporated off under vacuum. The precipitate formed during the evaporation is drained by suction, washed with EtOAc and dried. 7.89 g of the expected compound are obtained.

後処理

  1. concentrationThe reaction mixture is partially concentrated under vacuum
  2. additionan EtOAc/water mixture is added
  3. customthe phases are separated
  4. washthe organic phase is washed with saturated NaCl solution
  5. dry with materialdried over MgSO4
  6. customthe solvent is evaporated off under vacuum
  7. customThe precipitate formed during the evaporation
  8. washwashed with EtOAc
  9. customdried

出典と根拠

ORDレコード
ord-db652a6b705346deb2812c9a881d2ec1
出典データセット
uspto-grants-2015_08
特許番号
US09115121B2

関連ノート

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